Preparation and imidization method of polyimide hollow fiber membrane

A technology of polyimide and fiber membranes, applied in the field of polyimide hollow fiber membranes, can solve problems such as planarity and symmetry destruction, achieve a smooth and symmetrical segment structure, improve the degree of cyclization, and improve the degree of imidization Effect

Inactive Publication Date: 2020-02-07
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Thermal imidization is more commonly used, but the polyamic acid chain will rotate and translate during high temperature dehydration and ring formation, which will destroy the planarity and symmetry of the chain

Method used

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  • Preparation and imidization method of polyimide hollow fiber membrane
  • Preparation and imidization method of polyimide hollow fiber membrane
  • Preparation and imidization method of polyimide hollow fiber membrane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1) PMDA and ODA are added in DMAc, stir, obtain the polyamic acid solution that solid content is 15%.

[0035] (2) The polyamic acid hollow fiber membrane was prepared from the polyamic acid solution by dry jet wet spinning, and then soaked in deionized water for 8 hours to make it completely solidified. After solidification, put it into a solvent with a small surface tension for solvent exchange, and soak for 20 hours.

[0036] (3) Put the prepared polyamic acid hollow fiber membrane into a system composed of dehydrating agent acetic anhydride, catalyst pyridine and triethylamine, and soak at a temperature of 30-100° C. for 20 h.

[0037] (4) Wrap the polyimide hollow fiber membrane after solvent exchange with aluminum foil and put it in an oven, raise the temperature from room temperature to 135-180°C, keep it warm for two hours to remove the solvent, and continue to heat up to 300-360°C to make it sub- Amination is complete.

[0038] (5) The morphology of the poly...

Embodiment 2

[0043] (1) Add BPDA and ODA into DMAc, stir to obtain a polyamic acid solution with a solid content of 15%.

[0044] (2) The polyamic acid hollow fiber membrane was prepared from the polyamic acid solution by dry jet wet spinning, and then soaked in deionized water for 8 hours to make it completely solidified. After solidification, put it into a solvent with a small surface tension for solvent exchange, and soak for 20 hours.

[0045] (3) Put the prepared polyamic acid hollow fiber membrane into a system composed of dehydrating agent acetic anhydride, catalyst pyridine and triethylamine, and soak at a temperature of 30-100° C. for 20 h.

[0046] (4) Wrap the polyimide hollow fiber membrane after solvent exchange with aluminum foil and put it in an oven, raise the temperature from room temperature to 135-180°C, keep it warm for two hours to remove the solvent, and continue to heat up to 300-360°C to make it sub- Amination is complete.

[0047] (5) The polyimide hollow fiber m...

Embodiment 3

[0049] (1) Add 6FDA and ODA to DMAc and stir to obtain a polyamic acid solution with a solid content of 15%.

[0050](2) The polyamic acid hollow fiber membrane was prepared from the polyamic acid solution by dry jet wet spinning, and then soaked in deionized water for 8 hours to make it completely solidified. After solidification, put it into a solvent with a small surface tension for solvent exchange, and soak for 20 hours.

[0051] (3) Put the prepared polyamic acid hollow fiber membrane into a system composed of dehydrating agent acetic anhydride, catalyst pyridine and triethylamine, and soak at 30-100° C. for 20 h.

[0052] (4) Wrap the polyimide hollow fiber membrane after solvent exchange with aluminum foil and put it in an oven, raise the temperature from room temperature to 135-180°C, keep it warm for two hours to remove the solvent, and continue to heat up to 300-360°C to make it sub- Amination is complete.

[0053] (5) The polyimide hollow fiber membrane morpholog...

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Abstract

The invention provides a preparation and imidization method of a polyimide hollow fiber membrane. The preparation and imidization method comprises the steps that firstly, a polyamide acid hollow fibermembrane is prepared through a dry-spraying wet-spinning method, after the coagulation is completed, an original solvent (DMAc) and residual liquid (deionized water) in coagulating bath are exchangedby solvent exchange, then a nascent fiber membrane is immersed in an imidization reagent to be cyclized at low temperature, then after the partially immersed cyclized polyamide acid hollow fiber membrane is put into an oven for heating to remove the solvent, and is continuously heated for fully imidization. According to the preparation and imidization method, polyamide acid can be partially cyclized at the low temperature firstly, the chain structure is fixed, the transfer and rotation is prevented in the subsequent heating process, the defects of the hollow fiber membrane can be effectivelylowered, and the key performances of mechanical property, pressure resistance, gas permeability and separation performance and the like of the hollow fiber membrane can be improved.

Description

technical field [0001] The invention belongs to the technical field of polyimide hollow fiber membranes, and in particular relates to an imidization method of a polyimide hollow fiber membrane using chemical imidization and thermal imidization mixed. [0002] technical background [0003] Polyimide materials have high strength and high modulus, good temperature resistance and excellent mechanical properties, low dielectric properties, radiation resistance, chemical stability, and good resistance to electron radiation, and some polyimide Amines have good biocompatibility and are self-extinguishing polymers. Because polyimide has many excellent properties mentioned above, its development prospect is extremely broad. [0004] Due to the dependence on fossil energy, the number of factories relying on coal for energy has gradually increased, releasing a large amount of CO 2 into the air, which contributes to global warming. The purification of gas is particularly important. Mos...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D71/64B01D69/08B01D69/02B01D67/00B01D53/22
CPCB01D53/228B01D67/0006B01D69/02B01D69/08B01D71/64
Inventor 武德珍李依浓牛鸿庆朱丽
Owner BEIJING UNIV OF CHEM TECH
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